摘要
目的:建立测定荆芥挥发油中6种单萜类化合物(β-香叶烯、D-柠檬烯、薄荷酮、薄荷呋喃、胡薄荷酮、β-石竹烯)含量的方法。方法:采用气相色谱-质谱联用技术。色谱柱为HP-5MS毛细管柱(30m×0.25mm×0.25μm),载气为氦气,载气流速为1.0ml/min,进样口温度为220℃,程序升温;离子源为电轰击电离源,电子能量为70eV,离子源温度为230℃,四级杆温度为150℃,接口温度为280℃,质量扫描范围为40～400amu。结果:β-香叶烯、D-柠檬烯、薄荷酮、薄荷呋喃、胡薄荷酮和β-石竹烯的质量浓度分别在0.00318～0.03180、0.04226～0.42260、0.35168～3.51680、0.01934～0.19340、0.61120～6.11200、0.00798～0.07980mg/ml范围内与各自峰面积积分值呈良好的线性关系(r分别为0.9993、0.9998、0.9994、0.9997、0.9999、0.9995);精密度、重复性、稳定性试验的RSD均<3%;平均加样回收率分别为99.22%、98.34%、98.05%、97.56%、98.22%、99.06%,RSD分别为0.86%、0.92%、2.28%、1.21%、1.61%、1.17%(n均为6)。结论:该方法专属性强、准确度高、重复性好,可用于荆芥挥发油的质量控制。
OBJECTIVE： To establish the method for the content determination of 6 monoterpenoids（fl-myrcene, limonene, mcnthone, menthofuran, pulegone and β-caryophyllene） in volatile oil of Schizonepetae tenuifolia. METHODS： GC-MS method was adopted. A HP-SMS（30m×0.25mm×0.25μm） column was used with helium as carrier gas at flow rate of 1.0 ml/min. The injector temperature was 220 ℃ by temperature programming. Mass spectrometer conditions were： ionization mode： El, electron energy 70 eV, ion source temperature： 230 ℃; quadropole temperature： 150 ℃, interface temperature： 280 ℃, mass scan range： 40-400 ainu. RESULTS： The linear ranges β-myrcene, limonene, menthone, menthofuran, pulegone and β-caryophyllene were 0.003 18-0.031 80 mg/ml（r=0.999 3）,0.042 26-0.422 60 mg/ml（r=0.999 8）,0.351 68-3.516 80 mg/ml（r=0.999 4）,0.019 34-0.193 40 mg/ml （ r= 0.999 7 ）. 0.611 20-6.112 00 mg/ml （ i.= 0.999 9 ） and 0.007 98-0.079 80 mg/ml （r= 0.999 5 ）, respectively. RSDs of precision test. reproducibility test and stability test were all lower than 3%.The average recovery rates were 99.22%, 98.34%, 98.05%, 97.56%,9H.22% and 99.06% ,and RSDs were 0.86%,0.92%,2.28%,1.21%, 1.61%, 1.17%（n=6）.CONCLUSION： Theestablished method has strong specificity, high accuracy and good reproducibility. It can be used for quality control of volatile oil of S. temdfolia.
出处
《中国药房》
CAS
CSCD
2013年第15期1377-1379,共3页
China Pharmacy
基金
国家中医药管理局中医药行业科研专项资助课题(No.201007012-1-7)
江苏省中医药局科技项目资助(No.LZ11118)
江苏高校优势学科建设工程资助项目(No.ysxk-2010)
南京中医药大学中药学一级学科开放课题(No.2011ZYX1-009)
关键词
荆芥挥发油
单萜
气相色谱-质谱联用技术
含量测定
Volatile oil of Schizonepetae tenuifolia
Monoterpenoids
GC-MS
Content determination
